甘遂定量指纹图谱研究及响应面法优选醋制甘遂的炮制工艺

Study of Full-Quantified UPLC Fingerprint and Optimal Process of Effective Constituents from Kansui Radix Processed with Vinegar by Response Surface Method

目的:建立并比较不同产地甘遂UPLC指纹图谱,并同时测定指标成分大戟二烯醇的含量;在此基础上对甘遂醋制工艺参数进行了优选。方法:色谱条件包括流动相为乙腈-0.1%甲酸水溶液(梯度洗脱)、检测波长为210 nm、流速为0.4 m L/min、柱温35℃;建立10批不同产地甘遂药材UPLC指纹图谱,对10批样品的相似度进行评价,并且测定大戟二烯醇含量;以大戟二烯醇和醇浸出物含量的综合评分为因变量,运用Box-Behnken试验考察加醋量、炒药温度、炒制时间对醋甘遂炮制工艺的影响,运用Design Expert 8.05软件对试验数据进行分析,确定醋甘遂的炮制工艺参数。结果:确定共有指纹峰14个,除一批来自山西的药材外,相似度均大于0.94;确定醋甘遂的炮制工艺参数为每100 g药材加醋40%,265℃,炒制7 min。结论:本实验建立的甘遂指纹图谱及大戟二烯醇含量测定方法有较强的针对性,优选的醋甘遂炮制工艺方法可行,为甘遂药材的安全性研究以及制定甘遂饮片的质量控制标准提供了科学依据。

Objective ： To establish full - quantified UPLC fingerprint and optimal process of effective constituents from Kansui Radix processed with vinegar by response surface method. Methods ： The mobile phases were acetonitrile and 0.1% formic acid - water eluting in a linear gradient mode at the flow rate of 0.4 mL · min, the column temperature was 35℃ and the wavelength of UV detection was 210 nm. Ten batches of Kansui Radix samples from different habitats were determined and the characteristic spectra of those were established. The content of euphol was also determined simultaneously. And then according to synthetic gra- ded value of euphol and extract of vinegar processed Kansui Radix for index, Box - Behnken experimental design was adopted to investigate the effects of three main factors including dosage of vinegar, temperature and time of fried medicine. Experimental data analysis was disposed by Design Expert 8.05 software, multivariate quadratic regression equation mathematical model between synthetic graded value and independent variables was established, and then technical parameters were determined by response sur- face method. Results ： Fourteen common peaks were selected as makers in UPLC fingerprint of ten batches of samples of Kansui Radix, and the overall similarity was good according to the similarity calculation. Based on the results of response surface method, the best processing technology parameter was ascertained as follows：dosage of vinegar was 40%, temperature was 265 0（;, time of fried medicine was 7 min. Conclusion ： Fingerprint and quantitative analysis of Kansui Radix was satisfactory and specific, the suit- ability of surface method in optimizing processing technology of vinegar processed Kansui Radix. Established methods provided scientific basis of quality control specification and medication safety for Kansui Radix in the future.